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MoS2: a Choice Substrate for Accessing and Tuning the Electronic
Properties of Graphene
Chih-Pin Lu1,2
, Guohong Li1, Li-Min Wang
2, K. Watanabe
3, T. Taniguchi
3 and Eva Y.
Andrei1
1 Department of Physics and Astronomy, Rutgers University, Piscataway, New Jersey
08855, USA
2 Department of Physics, National Taiwan University, Taipei 10617, Taiwan
3National Institute for Materials Science, 1-1 Namiki, Tsukuba, 305-0044,
Japan
Research into the electronic properties of graphene and its viability for device
applications has fueled an ongoing quest for substrate materials that are minimally
invasive. While graphite was found to be perfectly suited for shielding graphene from
external perturbations, its metallic screening precludes control of the carrier density
by gating, which renders it unsuitable for device applications. Another candidate,
hBN, which is atomically flat, chemically inert, and allows gating, can cause
significant bandstructure reconstruction in graphene due to the close match of their
atomic structures. Here we report on the suitability of MoS2 substrates as measured by
scanning tunneling microscopy and Landau level spectroscopy in a device
configuration which allows tuning the carrier density of graphene by gating. We find
that, similarly to hBN, graphene on MoS2 is ultra-flat producing long mean free paths
and sharp Landau levels down to magnetic fields of 2T, while completely avoiding
the band structure reconstruction caused by hBN. Importantly, we find that the
screening properties of the MoS2 substrate can be tuned with relatively low gate
voltages from insulating to metallic leading to a substantial increase in the scattering
length. The use of MoS2 substrates thus provides unique opportunities to access the
intrinsic electronic properties of graphene and to study in situ the effects of screening
on electron-electron interactions and transport.
The vulnerability of atomically thin layers such as graphene1-3
to environmental
disturbances has prompted an ongoing search for substrates that can support the
material without perturbing its electronic structure. Graphite substrates were found to
be by far the least invasive, making it possible to observe the intrinsic low energy
spectrum of graphene by using scanning tunneling microscopy (STM), spectroscopy
(STS)4-7
, and cyclotron resonance (CR)8 measurements. Landau level spectroscopy
showed that on graphite substrates the quasiparticle lifetime in graphene is intrinsic,
originating from electron-electron interactions, with the only source of external
scattering being the sample boundaries5. In this sense graphite substrates are ideally
suited for accessing the low energy spectrum of graphene. However the strong
metallic screening of bulk graphite, which precludes control of the carrier density by
gating and masks the electron-electron interactions, imposes severe limitations for
both applications and fundamental studies. The alternative is to use insulating
substrates, but the versatility gained comes at the price of enhanced sensitivity to
surface corrugations 9-11
and impurities12-16
, which create electron-hole puddles that
obscure the low energy electronic properties at the Dirac point17
. These perturbations
can be mitigated by the use of atomically flat18
and chemically inert substrates such as
hexagonal boron nitride (hBN)19-22
. However the close match between the lattice
structure of graphene and the substrate leads to a spatial modulation which
significantly perturbs the electronic spectrum by producing Van-Hove singularities23,
24, band gaps
25 and new sets of Dirac cones
26-30. Here we show that atomically flat
MoS2 substrates provide access to the intrinsic band structure of graphene while at the
same time allow tuning via a gate voltage both the carrier density and the strength of
screening.
MoS2 is a semiconductor in the layered transition metal dichalcogenite family
consisting of covalently bonded S-Mo-S sheets held together by the van der Waals
force. Its weak interlayer coupling facilitates the extraction of ultra-thin layers by
exfoliation. Bulk MoS2 has an indirect bandgap of 1.2~1.3eV31
which, due to
quantum confinement, crosses over to a direct bandgap of ~1.9eV when the material
is exfoliated down to a monolayer32
. Thin layers of MoS2 are well suited to serve as
the channel material in FET applications, exhibiting high room temperature mobility,
almost ideal switching characteristics, and low standby power dissipation33-36
. The
fact that the position of the Femi energy can be promoted from the gap to the
conduction band with relatively modest gate voltages, allows tuning the screening
properties of MoS2 films from insulating to metallic. Further, the absence of dangling
bonds and of surface states renders its surface inert, clean and minimally invasive.
The large lattice mismatch between MoS2 and graphene, together with its chemical
inertness and the tunable screening, renders MoS2 ideally suited as a substrate
material for studying graphene by STM and STS.
We employed thin MoS2 flakes that were exfoliated from commercial 2H-MoS2
crystals (SPI CAS # 1317-33-5) and deposited onto a 300nm chlorinated SiO2
substrate37
capping a degenerately p-doped Si gate. The flakes were identified by
optical microscopy and their thickness was measured using atomic force microscopy
(AFM) in ambient conditions. Subsequently a flake of graphene which was exfoliated
from bulk HOPG and deposited on a thin PMMA film was optically aligned with the
MoS2 substrate and pressed onto it while heating the sample stage to ~100 oC
19 . We
employed e-beam lithography followed by electron-beam evaporation at a base
pressure of 2×10-7
Torr to prepare the Ti/Au (3nm/70nm) contacts. Similar methods
have been used to prepare samples on hBN substrates. As for grapheme on SiO2,
graphene was deposited directly without the special alignment process. The devices
were baked for 3hrs in forming gas (90% Ar, 10% H2) at 250 oC prior to performing
STM measurements in a home-built STM operating at temperatures down to 4K and
in magnetic fields up to 12T. Coarse X-Y motors were used to locate the micron sized
sample38
. Figure1(a) illustrates the measurement set up and electrode configuration
for the gated STM/STS studies. The images were acquired in constant current mode
with the bias voltage, Vb, applied to the sample and using Pt-Ir tips mechanically cut
from a polycrystalline wire. Differential conductance, dI/dV which is proportional to
the local density of states (LDOS) 39
, was measured with lock-in detection at
frequency f = 440Hz with fixed tip to sample distance. The gate voltage, Vg, was
applied between the Si backgate and the sample. This measurement configuration
which combines STS with gating capabilities makes it possible to study the effect of
screening on the electronic properties of graphene.
Figures 1(b-e) show STM topography images, 80nm × 80nm in size, of graphene
on several substrates: MoS2 (b), SiO2 (c) and hBN (d,e). In Figure 1(f) we compare
the height profile on these substrates taken along the lines indicated in the topography
images. Since graphene tends to conform to the substrate its corrugation on atomically
flat surfaces such as MoS2 or hBN is naturally much smaller than on amorphous
surfaces such SiO2. Indeed we find that the average surface corrugation of graphene
on hBN (0.1nm), as shown in Figure 1(d), is one order of magnitude smaller than on
SiO2 (0.9 nm), consistent with earlier reports9, 20, 21
. This is in marked contrast to the
case shown in Figure 1(e) where in spite of the atomically flat hBN substrate the
surface exhibits a large periodic corrugation with an apparent height of ~0.4nm. The
stark difference between the images in Figures 1(d) and 1(e), both showing the
topography of graphene on hBN, is due to different relative twists between the lattice
orientations of graphene and hBN. The relative twist angle, together with the lattice
mismatch, aBN/a ~ 1.8% between graphene and hBN gives rise to a moire
superstructure of period20
2)cos1)(1(2
)1(a
where aBN and a are the
lattice constants of hBN and graphene respectively. The superstrtucture in Figure 1(e)
is due to the small twist angle, ~0.1o, which gives rise to the large periodic modulation
in topography and in the LDOS. In contrast, the twist angle in Fig. 1(d) is too large
(>20o) to produce a measurable superstructure resulting in the much smoother
appearance. Thus, substrates with lattice structures closely matched to that of
graphene (small ) such as hBN4 or a second layer of graphene
23, can produce a large
disturbance in the band structure, even when they are atomically flat. In contrast, for
substrates with large mismatch such as MoS2 the disturbance is minimal.
Figure 2 shows the evolution of the dI/dV spectra with gate voltage for graphene
deposited on a ~30nm thick MoS2 substrate. All energy measurements are referred to
the Fermi energy (EF), which is the zero of energy. Determining the position of the
DP from the zero field LDOS of graphene on an insulating substrate is a challenging
task7 because the inevitable presence of electron-hole puddles smears out the
minimum at the DP. Furthermore, in the absence of screening the zero-bias anomaly
produces a pronounced minimum which can overshadow the minimum at the DP7, 40
.
The arrows in Fig. 2(a) at the center of the broad minimum are a rough estimate of the
DP position. This choice was guided by the finite field data (Figure 4) where the
position of the DP is much less ambiguous. This is because in a magnetic field the
center of the N=0 Landau level (LL) coincides with the DP and the position of EF
coincides with its zero field value for Vg corresponding to a half filled LL7. Plotting
the gate voltage dependence of ED in Fig.2(b) we find that for Vg < 10V the data
qualitatively follows the massless Dirac fermion spectrum expected for graphene:
√ | |. Here V0 ~ 4.5V represents the voltage to compensate the
unintentional doping, α≈ 6.6 × 1010
cm-2
V-1
is the carrier density per volt of gate
voltage and vF =1.21 2×106 m/s is the Fermi velocity. The values of αand vF
were obtained from the LL spectra as discussed below. We note that the for Vg >
−10V the gate dependence of ED is significantly slower, indicating that most of the
gate induced charge is taken up by the MoS2 substrate. Indeed from the finite field
data we find that in this regime only ~25% of the gate induced charge goes the
graphene layer, the rest being absorbed by the MoS2 substrate. This suggest that EF
has entered the conduction band (CB) of MoS2 21
at which point the gate induced shift
in the position of ED is determined by the LDOS of the combined graphene/MoS2
system, as illustrated in the inset of Figure 2(b). Since the LDOS in the CB of MoS2 is
larger than that of graphene most of the charge is absorbed by the former. For
comparison we show in Figure 2(b) the gate dependence of ED for graphene deposited
on chlorinated SiO2 which remains insulating for all values of the applied Vg. In this
case the gate induced charge populates only states in graphene resulting in the
expected square-root gate dependence of ED for the entire range of applied Vg. For the
chlorinated SiO2 substrate we find α≈ 7.3 × 1010
cm-2
V-1
, V0 ~ 12V and vF
=1.1 2×106 m/s .
In the presence of a perpendicular magnetic field the dI/dV spectrum breaks up
into a sequence of LL peaks. The evolution of the LLs with magnetic field for
graphene on MoS2 and on chlorinated SiO2 at Vg = 10V is shown in Figures 3(a) and
3(b). In both cases the LL sequence follows the field and level index (N) dependence
characteristic of massless Dirac fermions as expected for single-layer graphene 2:
( )√ | | (1)
Here e is the magnitude of the electron charge and N > 0 (N < 0) corresponds to
electron (hole) levels. Fitting the measured sequence of energy levels to this
expression we obtain vF =1.21 0.02 ×106 m/s and vF =1.1 0.02 ×10
6 m/s for
graphene on MoS2 and chlorinated SiO2 respectively. One of the prerequisites for
observing well developed LLs is for the random potential to be smooth on the length
scale of the cyclotron orbit, ( ) √
√ . Therefore the field at which LLs
become resolved signals that the cyclotron orbit is sufficiently small to “fit” within
the characteristic puddle size of a particular sample37
. For graphene on MoS2, Figure
3(a), the LLs are already well resolved at 2T indicating that the characteristic puddle
size exceeds ( ) . For the case of graphene on chlorinated SiO2, Figure
3(a), LLs become distinguishable at 6T, indicating smaller puddles bounded by
( ) . The electron-hole puddles can be directly imaged through dI/dV
maps representing the spatial dependence the local doping. Figures 3(c) and (d) show
the maps of the N = 1 LL energy at 10T for graphene on the MoS2 and chlorinated
SiO2 substrates respectively. The spatial fluctuations in the map reflect local substrate
induced hole (blue) doping for negative energy shifts and electron (red) doping for
positive energy shifts. For the MoS2 substrate the average puddle size obtained from
the color maps ~ 30nm, slightly larger than the values reported for graphene on hBN
22, suggests that LL would remain well resolved down to magnetic fields of 0.5T. The
average puddle size for the chlorinated SiO2 substrate, ~10nm, is in good agreement
with that obtained from the LL spectra.
To study the effect of doping on the LLs we measured the gate dependence of
the dI/dV spectra at fixed field. The results for B = 8T and 10T (Supplementary
material S2) are summarized in the map shown in Fig4(a). Each vertical line
corresponds to the spectrum taken at a particular gate voltage. The pronounced
staircase features reflect the high degeneracy of the LLs each of which can
accommodate a carrier density of
= 10
11B[T] states/cm
2, where = 4.14 x
10-11
Tcm2, is the fundamental unit of flux. In the process of gating, each LL pins the
Fermi energy as it is filled causing the plateau features. The width of a plateau, Vg=
D/, reflects the gate voltage required to supply D carriers per unit area to the
graphene layer. The bias-voltage dependent shifts in the step position appearing as
diagonal lines on the map are due to tip induced gating.
For the data in Fig 4(a) in the regime where the MoS2 substrate is insulating, Vg
< −10V, we find Vg = 11.8V which gives 6.6 × 1010
cm-2
V-1
. For Vg > −10V,
the plateaus become much wider with Vg ~ 50V and 1.5 × 1010
cm-2
V-1
indicating that EF has entered the CB of MoS2. At this point ~75% of the carriers
introduced by the gate are taken up by the MoS2 substrate which can now provide
better screening of the random potential (Supplementary material S2).
In Figure4(b) we present the LL spectra for several values of Vg. Fitting in
Figure 4(c) the energies of the LLs obtained from these spectra with Eq. (1), we find
vF ~ (1.21 0.5) ×106 m/s. Furthermore, as shown in the inset, we find no systematic
gate dependence of vF. Since vF, is inversely proportional to the dielectric constant41
this implies that, in spite of the increased screening accompanying the entry of EF into
the conduction band, the dielectric constant of MoS2 does not depend on doping for
the range of Vg employed here, consistent with recent theoretical work42
. This value
of vF is comparable to that obtained on the chlorinated SiO2 substrate whose dielectric
constant ~4 is close to that of MoS2.
To illustrate the effect of screening we compare in Figure 4(d) the linewidth, E,
of the N=0 LL in the unscreened (Vg = 30V) and screened regimes (Vg = +25V).
Using a Gaussian fit we find E ~ 54mV for the unscreened case, which corresponds
to a quasiparticle lifetime of E/ = 12fs and to a scattering length of lmfp~
vFnm. In the screened regime we find a much narrower linewidth, E ~ 28mV,
indicating a significant reduction in scattering with correspondingly longer
quasiparticle lifetimes ~23fs and a mean free path of lmfp ~ 28nm. Interestingly the
mean free path obtained from the N=0 LL linewidth is comparable to the average
puddle size, in Figure 3(c), indicating that the electron-hole puddles are the main
scattering source in graphene. A similar analysis of the N=0 LL on chlorinated SiO2
(Figure 3b) gives a quasiparticle lifetime of ~ 10fs and lmfp~ 11nm comparable to
the puddle sizes in this system, so that here too electron-hole puddles are the main
source of scattering.
In summary, the quality of MoS2 substrates as measured by the quasiparticle
mean free path is remarkably good: in the unscreened regime it is comparable to that
in the best insulating substrates, hBN and chlorinated SiO2, while in the screened
regime it is larger still. The results presented here demonstrate that MoS2 substrates
are perfectly suited for accessing the low energy electronic properties of graphene
while at the same time providing great flexibility through controllable carrier densities
and tunable screening.
Acknowledgements
Funding was provided by DOE-FG02-99ER45742 (E.Y.A, G.L) , NSF DMR
1207108 (E.Y.A. , C.P.L) and National Science Council of Taiwan (C.P.L)
Figure 1. (a) Schematic of graphene on multilayer MoS2 substrate with gating
capabilities. The sample bias Vb is applied between the STM tip and the sample
contacted by a Ti/Au electrode. The edge of the graphene flake is marked by the
dashed line. The back gate voltage Vg is applied between the Si substrate and the top
electrode. (b)(c) Constant current STM topography image of graphene on MoS2 and
on chlorinated SiO2 respectively. The area of both images is (80nm×80nm) (d)(e)
Constant current STM topography image of graphene on BN(80nm × 80nm) with and
without moire pattern, respectively. (f) Profile line of Section view through (b),(c),(d)
and (e) indicating the corrugation of graphene on MoS2 (black), graphene on SiO2 (red)
and graphene on BN(blue) and graphene on BN with moire pattern(green). The
tunneling conditions were: Iset=20pA and Vb=0.4V. The Insets in (b-d) represent
zoom-in images to atomic resolution with scale bar of 0.3nm.
.
Figure 2. (a) dI/dV measurements of graphene on MoS2 taken at the same position for
different gate voltages. Curves are vertically displaced for clarity. Arrows indicate the
position of the Dirac point as discussed in the text. Measurement parameters: set point
current I = 20pA at Vb = 0.35V, AC modulation 5mVrms. (b) The Dirac point as
function of gate voltage for graphene on MoS2 (blue squares) and graphene on SiO2
(red squares). The solid lines represent the simulated gate dependence of the Dirac
point in the regime where the substrate is insulating. The top inset represents the
density of states of graphene on an insulating substrate. The bottom inset shows the
combined density of states of graphene (red) and the MoS2 substrate (teal) together
with the resulting gate dependence of the Dirac point energy as described in the text.
Figure 3. Magnetic field dependence of STS dI/dV spectra. (a),(b) Landau level
spectra for several magnetic fields and Vg= 10V for graphene on MoS2 and on SiO2,
respectively. The LL indices N = 0, ± 1, ±2..... are marked. STS parameters: set point
I=20 pA, Vb=0.35V, AC modulation 2mVrms. The lower panels are histogram of the
height distribution measured by AFM of MoS2, graphene on MoS2, SiO2 and
graphene on SiO2 as marked. (c),(d) Spatial variation of the N= 1 LL peak position
in B=10T obtained from a dI/dV map at Vg =0V representing the doping
inhomogeneity in graphene. STS parameters: set point I= 20pA, Vb= 0.35V, AC
modulation 2mVrms
Figure 4. (a) Gate map of the dI/dV spectra at 8 T. Each vertical line in the map
corresponds to a LL spectrum at a particular gate voltage. White stripes correspond to
the LL peaks energies as indicated by N = 0, ± 1, ±2.... STS parameters: set point
current I= 20 pA, Vb=0.4V, AC modulation 5mVrms. (b) LLs at Vg= 28V, 14V,
20V and 12V. (v) Solid dots are data points and the line represents a fitting for LLs of
graphene on MoS2 in B= 8T at Vg= 28V, 14V, 20V and 12V. Inset: Gate
dependence of Fermi velocity at Vg = 30~25V.(d) The Solid squares are data points
and the line represents a fitting for LLs N=0 with Gaussian at Vg=30V and 25V.
The curves are offset for clarity.
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